3 lines
6.3 KiB
JSON
3 lines
6.3 KiB
JSON
{
|
||
"protocol": "The hydrophilic polymer is synthesized using a two-component system comprising a first oligomer and a second oligomer. The first component oligomer includes: (a) 20 to 99 parts by weight of polymerized monomer units derived from an ethylenically-unsaturated monomer possessing a poly(alkylene oxide) group, (b) 0.1 to 35 parts by weight of polymerized monomer units derived from an ethylenically-unsaturated monomer with a pendent polymerizable group, (c) 0 to 50 parts by weight of polar monomer units, and (d) 0 to 20 parts by weight of hydrophobic monomer units. The second component oligomer consists of: (a) 0.01 to 99.99 parts by weight of free radically polymerizable monomer units and (b) 99.99 to 0.01 parts by weight of polymerized monomer units derived from an ethylenically-unsaturated monomer having a pendent photoinitiator group. The two components should be combined such that the second component provides greater than two crosslinks per first component oligomer chain upon curing. Polymerization can be conducted through thermal or photochemical methods using appropriate solvents and initiators. For photoinitiation, a variety of UV light sources and photoinitiators, as well as their optimal concentrations, are specified to achieve desired crosslinking and material properties.A series of hydrophilic copolymers were synthesized by charging 5 amber glass bottles with different weight proportions of hydrophilic monomers and alpha-methyl styrene. Sufficient ethyl acetate was added to each bottle so that the total monomer concentration was 50 weight percent. VAZO 52 (0.4 g) was added to each bottle. The contents of each bottle were purged with nitrogen gas for 20 minutes and the bottle was capped using poly(tetrafluoroethylene) thread tape. Each bottle was placed in a Model LLF LAUNDER-O-METER, with the water bath temperature set at 60°C, for 16 hours. After 24 hours, each sample disk was removed from the solution and the excess liquid was allowed to drip off for 1 minute. The sample disk was weighed and this weight was recorded as \"wet weight.\" The absorbency of each sample disk was calculated as the increase in sample weight, expressed as a percentage of the dry weight.A hydrophilic copolymer with photoinitiator pendant groups was synthesized by charging an amber glass bottle with 99.0 g of MPEG, 1.0 g of DAROCUR ZLI-3331, 0.1 g of α-methyl styrene, 0.4 g of VAZO 52 and 100 g of ethyl acetate. The contents of the bottle were purged with N2 for 20 minutes and the bottle was capped, using poly(tetrafluoroethylene) thread tape between the cap and the threads of the bottle. The bottle was placed in a Model LLF LAUNDER-OMETER, with the water bath temperature set at 60°C, for 16 hours. The resulting polymer had a Mn of 36,900 as determined by GPC.Charge an amber glass bottle with 65.0 g of MPEG, 35.0 g of HEMA, 1.0 g of DAROCURE ZLI-3331, 4.0 g of alpha-methylstyrene, 0.4 g of AIBN, and 90 g of ethyl acetate. Purge the contents with nitrogen gas for 20 minutes and cap the bottle using poly(tetrafluoroethylene) thread tape. Place the bottle in a water bath shaker at 65°C for 24 hours. The resulting polymer has a Mn of 15,700 as determined by GPC.Each solution of the products from Preparatory Examples 3-7 was combined with VDM and a catalytic amount of DBU in an amber bottle. The bottle was agitated in a heated shaker water bath at 60°C for 16 hours.Each solution of the products from Preparatory Examples 3-5 was combined with IEM and a catalytic amount of dibutyltin dilaurate in an amber bottle. The bottle was agitated in a heated shaker water bath at 60 degrees C for 16 hours.A series of hydrophilic copolymers were synthesized by charging 4 amber glass bottles with different weight proportions of hydrophilic monomers and alpha-methyl styrene, and VAZO 52 (0.4 g). Sufficient ethyl acetate was added to each bottle so that the total monomer concentration was 50 weight percent. The contents of each bottle were purged with nitrogen gas for 20 minutes and the bottles were capped using poly(tetrafluoroethylene) thread tape. Each bottle was placed in a Model LLF LAUNDER-O-METER, with the water bath temperature set at 60 degrees Celsius, for 16 hours. This step was performed by agitating the mixture at room temperature for 48 hours.Combine solutions of products from Preparatory Examples 16-19 with different proportions of HEMA, BHT (100 ppm), and a catalytic amount of DBU in an amber bottle. Agitate the bottle in a heated shaker water bath at 60°C for 16 hours.A hydrophilic copolymer was synthesized by charging an amber glass bottle with 65.1 g of MPEG, 35.0 g of HEMA, 4.0 g of a-methyl styrene, 0.4 g of AIBN and 90 g of ethyl acetate. The contents of the bottle were purged with nitrogen gas for 20 minutes and the bottle was capped, using poly(tetrafluoroethylene) thread tape. The polymerization bottle was placed in a water bath shaker at 65°C for 24 hours. The resultant polymer had a M_n of 12,200 as determined by GPC. A series of copolymers with pendent ethylenic unsaturation were prepared by reacting portions of this copolymer with different weight proportions of IEM and a catalytic amount of dibutyltin dilaurate.A series of films were prepared by mixing either IG184 or different proportions of the solution of the product of Preparative Example 1 (referred to as Component C) with different proportions of each solution of the product of Preparative Examples 20-23 (referred to as Component D). The mixed solutions were separately coated onto poly(ethylene terephthalate) (PET) release liner and the solvent was evaporated by heating the coatings in an oven at 50°C for 4 hours. Another layer of PET release liner was then placed on top of the film, providing a coated film between two sections of PET release liner. This was irradiated as described in previous examples.A series of films were made by mixing equal weights of a solution of each of the products from Preparative Example 24-29 (identified as Component E in Table 9) with a solution of the product of Preparative Example 2. The resultant solutions were separately coated onto poly(ethylene terephthalate) (PET) release liner, and the solvent was evaporated by heating the coatings in an oven at 50°C for 4 hours. Another layer of PET release liner was then placed on top of the film, providing a coated film between two sections of PET release liner. This was irradiated as described in Examples 30-61."
|
||
} |